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Angular momentum resolved EELS by energy filtered nanobeam ...

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Simon D. Schneider, Cécile Hébert, Guillaume Lucas<br />

Centre Interdisciplinaire de Microscopie Electronique (CIME)<br />

Ecole Polytechnique Fédérale de Lausanne<br />

1015 Lausanne, Switzerland


¨<br />

¨<br />

¨<br />

¨<br />

<strong>Angular</strong> <strong>resolved</strong> <strong>EELS</strong><br />

Microscope setup<br />

Data analysis<br />

Conclusion<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 2


¨<br />

¨<br />

¨<br />

¨<br />

<strong>Angular</strong> <strong>resolved</strong> <strong>EELS</strong><br />

Microscope setup<br />

Data analysis<br />

Conclusion<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 3


Classic<br />

q-<strong>resolved</strong><br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 4


Bulk silver prepared <strong>by</strong> twin<br />

jet electropolishing<br />

Zone Axis: [2,1,2]<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 5


Energy Filtered Transmission Electron Microscopy<br />

ΔE<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 6


Evolution of the loss function in the <strong>energy</strong><br />

range 0-55 eV as a function of <strong>momentum</strong><br />

transfer q in (1 1 1) direction.<br />

A. Alkauskas et al., Ultramicroscopy 110 (2010) 1081–1086<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 7


¨<br />

¨<br />

¨<br />

¨<br />

<strong>Angular</strong> <strong>resolved</strong> <strong>EELS</strong><br />

Microscope setup<br />

Data analysis<br />

Conclusion<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 8


¨<br />

Challenges:<br />

¡ Energy resolution<br />

¡ <strong>Angular</strong> resolution<br />

¡ Whole <strong>energy</strong> plane<br />

¡ Dynamic<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 9


A. Alkauskas et al.<br />

Ultramicroscopy 110 (2010) 1081–1086<br />

0.917 eV<br />

TEM image spectrum,<br />

Sputtered Ag<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 10


Energy filter used as a filter (EFTEM)<br />

Sample<br />

Cross over (chromatic object plane)<br />

Image or diff. pattern on the SEA (achromatic object plane)<br />

Filter<br />

Achromatic image plane<br />

Chromatic image plane (spectrum, <strong>energy</strong> selecting slit)<br />

Filtered image or diffraction patern<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 11


Size of the diaphragma projected on the sample:<br />

SAA1: 1600 nm; SAA2: 800 nm; SAA3: 320 nm; SAA4: 160 nm<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 12


Energy dispersion is image-couled in diff mode<br />

=> <strong>EELS</strong> spectrum convolved with SAA<br />

SAA4: 1.9 eV<br />

SAA3: 2.4 eV<br />

SAA2: 5.9 eV<br />

FWHM with 80 cm CL<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 13


19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 14


TEM mode<br />

NBD mode<br />

TEM OLA3 SAA4<br />

0.917 eV FWHM<br />

NBD without diaphragm<br />

1.015 eV FWHM<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 15


TEM mode<br />

NBD mode<br />

TEM OLA3 SAA4<br />

NBD without diaphragm<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 16


0<br />

G<br />

G/2<br />

Sputtered Ag, 50 nm thick<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 17


Sputtered Ag, 50 nm thick<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 18


CCD camera<br />

Imaging plates<br />

Sputtered Ag, grain orientation [0,0,1]<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 19


Improvement of the technique (summary)<br />

NBED<br />

+ // illum. on small area<br />

+ No aperture needed<br />

beside CLA<br />

- Much more sensitive to<br />

alignment<br />

- More contamination<br />

Imaging Plates<br />

+ High dynamic range<br />

+ No cross-talk<br />

- Manual acquisition and<br />

stack combinaison<br />

- Long scanning time<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 20


19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 21


¨<br />

¨<br />

¨<br />

¨<br />

<strong>Angular</strong> <strong>resolved</strong> <strong>EELS</strong><br />

Microscope setup<br />

Data analysis<br />

Conclusion<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 22


B. Schaffer et al., Ultramicroscopy 106 (2006) 1129–1138<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 23


¨<br />

Problems to overcome in EFNBED<br />

¡ Microscope alignment<br />

¡ <strong>Angular</strong> resolution<br />

¡ Contamination<br />

¡ Energy resolution<br />

¡ Dynamics<br />

¡ Non-isochromaticity<br />

¡ Schaffer correction<br />

¡ Plural scattering<br />

Done<br />

Done<br />

Not yet done<br />

In progress<br />

Done<br />

In progress<br />

In progress<br />

In progress<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 24


Thank you for your attention!<br />

19.06.2012 Workshop on <strong>EELS</strong> in materials sciences, Uppsala (S) 25

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